Production of beryllium compounds



L. BURGESS.

PRODUCTION OF BERYLLIUM COMPOUNDS. APPLICATION map AUG.I6, 19'21.

1,41,527 a ente June 6,1922.

/ ATTORNEY.

Louis BURGESS, 0E BAYONNE, NEW JERSEY.

PRODUCTION OF BERYLLIUM COMPOUNDS.

Application filed August 16. 1921.

To all whom it may concern Be it known that 1, Louis BURGESS, a' citizen of the United States, residing at Bayonne, in the county of Hudson and State of New Jersey, have invented certain new and useful Improvements in the Production of Beryllium Compounds, of which the following is a specification.

My invention relates to new and useful improvements in the production of beryllium chlorid and substantially pure beryllium oxid, or that compound commonly known as beryllia.

Beryllium o'xid usually existsin the form of a crude ore known as beryl, which is a silicate containing approximately 12 to 15 per cent of beryllium oxid and 85 per cent silica (SiO together with traces of other oxids. Beryllium oxid (BeO) is relatively insoluble as it exists in beryl, in either acids or alkalies, unless the silica is eliminated as an alkali silicate by fusion with alkali, such as sodium carbonate or hydrate, or as a fluoride by the use of hydrofluoric acid. The amount of silica to be eliminated in this manner is so great and the methods are attended with such difficulty that they are not generally practised on an industrial scale.

My invention contemplates the provision of a process which will permit satisfactory and comparatively simple recovery of substantially pure beryllium oxid from the.

crude ore beryl, as will be fully set forth hereinafter.

According to the preferred form of my process, I take the crude ore beryl, which, as stated, is a silicate containing approximately 15 per cent of beryllium oxid and. 85 per cent silica. I then mix this pulverized beryl with a suitable hydrocarbon bonding agent, employing for this purposeabout 7 5 parts by weight of the said crude ore to about '50 parts by weight of the bonding agent. The bonding agent is preferably a high melting point pletroleum pitch, which, on heating, will yiel approximately 50 per cent of carbon. The ore may be mixed with the said pitch by any suitable means, care being taken to thoroughly pulverize and disseminate the ore throughout the body of pitch or bonding agent. I pref-. erably employa tub or pebble m1ll to pulverize and mix the ore and the bonding material and preferably pulverize the mass. I then cok'e the said mixture of beryl and Specification of Letters Patent.

Patented June 6, 1922.

Serial No. 492,822.

petroleum pitch by heating the same in a suitable retort to a red or yellow heat, and preferably in a reducing atmosphere. hen the mixture is properly coked, I grind the same, by any suitable means, until it is reduced to particles, say, of about a cubic inch maximum size.

The ground coked mixture of crude ore and carbon is then placed in an electric furnace. preferably operating on the are principle, and by the heat of the arc is reduced, the heating chamber in which, the reducing action is performed being maintained at a pressure of approximately 30 pounds to the square inch above atmospheric pressure. In performing the reducing step, I may use any suitable form of arc furnace capable of producing the desired temperatures and of maintaining the pressure mentioned, but for this purpose I preferably employ a furnace of the general type and construction shown in my application Serial No. 409,589, filed September 11, 1920. The resulting product is either a silicid (-Be si), or an alloy or compound of beryllium and silicon, depending upon the percentage of carbon in the coked mixture treated in the arc furnace. If more than 25 parts of carbon are used in proportion to the weight of the beryl, the beryllium will be partially or completely converted into beryllium carbid The resultant roduct, whether it be beryllium silicid v e Si) or beryllium carbid (Be C), is preferably ground to. a relatively fine condition, say, to pass a 50 to the inch mesh (or finer) screen and is then treated with dry gaseous hydrochloric acid in the presence of heat to convert the beryllium into anhydrous beryllium chlorid.

The reaction between the beryllium silicid, 0r beryllium carbid, and the dry hydrochloric acid gas is carried on in any suitable form of retort or furnace, as will be hereinafter described, and at or above a temperature at which the beryllium chlorid sublimes, namely, at a'temperature at least slightly below a red heat, i. e., about 450 0., said temperature being maintained during the reaction. At-.450 C., in the reaction vessel, any ferrous chlorid formed is involatile and will not enter the vapors leaving the reaction chamber. Itmay be, however, desirable to maintain a temperature in the reaction chamber at or about 800 C. (yellow heat) in order that any below the iron which may be present in the charge and is converted into ferrous chlorid (FeCl will be volatilized and pass out of thechamber. V Vapors of beryllium chlorid (BeCl are carried "off from the zone=of the reaction, the elemental silicon or carbon formed or resulting remainingin the reaction chamber. The silicon or a part of the same may be eliminated as gaseous silicon hydrid. The vapors evolved, and which pass from the zone of the reaction chamber, are led into a suitable condenser or settling chamber maintained at a temperature at or above the sublimation temperature of beryllium chlorid, namely, about 450 C.,- so that the same will not. be condensed in said condenser. Ferrous chlorid,

if present in the vapors, will be condensed out in the preliminary condensing or set- 'tling chamber, which, as stated, is maintained at approximately the sublimation temperature of beryllium chlorid, which is sublimation temperature of ferrous chlorid. The vapors of the beryllium chlorid from. which the ferrous chlorid has been separated may be carried on to another condensing chamber or a series of chambersmaintained at temperatures below that at which beryllium chlorid sublimes, and above the boiling or sublimation temperature of aluminum chlorid or zirconium chlorid, say, 200 C. or 250 (1., which results in condensation of a relatively .pure beryllium chlorid, the vapors of aluminum chlorid or zirconium chlorid, if present, passing on to another condenser or condensers, in which they; may be con densed and recovered as such; s

In order to produce the pure beryllium oxid, I then treat the beryllium chlorid re,

covered, in the manner described, with the theoretical amount of water necessary to apparatus is shown in elevation andvertical section, comprising a reaction chamber 1,

' lined with suitable fire-brick or refractory material 2, and to which the crude ore beryl is fed through an inlet duct 3 on the upper portion thereof, 4 designates a supply hopper to receive the finely divided carbid or silicid the said hopper opening at its lower end into a trough 5, in which is located a screw feed or conveyor 6 extending through said trough and through an outlet spout 7 which opens into the inletend of the feed duct- 3. The screw or spiral 6 is mounted on a shaft 8, in suitable bearings 9, and is driven by at suitable motor-10 through suitable transmission gearings 11. Surrounding the duct 7 is a feed duct 12 opening, as at 1 3, into the spout 3, said duct having an lnlet connection 14 to receive gaseous hydrochlonc acid which flows through the duct 12 and opening 13 into the p I passage 3, where it is intimately mixed with the finely divided beryl by means of agitator blades 15, mounted on the shaft 8.

\Vithin the chamber 2 are are electrodes 16 energized, in any suitable manner, -to heat the interior of the chamber to the' desired reaction temperature, namely, approximately 450 C. or above. The chamber may be provided with a suitable discharge, as shown at 17'.

The fumes of the beryllium chlorid, together with any other chlorids which may be volatil'ized in the reaction chamber, pass therefrom through a passage 18 into a preliminary condenser 19 containing a baflle '20, which condenser is maintained at approximately 450 C. so as to condense out any ferrous chlorid, if present, and permits the vol-atilized beryllium chlorid, and other;chlorids, if present, to pass on to the second condense-r, shown at- 21. This second condenser is maintained at a temperature, preferably above 200 C. and

below approximately 450 (1-, so that the beryllium chlorid will be condensed therein and may be recovered. The condenser 21 is provided with an ,outlet duct 22, through which any volatile products not condensed in condenser 21 may pass'to a third condenser'23, maintained also at a temperature above 200 to 250 C., and be low 450 C, so as to insure condensation and separation of any. beryllium chlorid which may not have been recovered in condenser 2'1. The condenser 23 is connected by a 'duct 24 with a final condenser 25,

maintained at a temperature below 150 C4, so as to condense out any aluminum chlorid or zirconium chlorid which may have been volatilized in the reaction chamber. It will be understood that most beryl ore contains small percentages of aluminum oxid, and in some instances percentages of zirconium oxid, and this final condensation is, therefore, necessary only if it is desired to recover the chlorids evolved in the reaction from these oxids. Any gases existin in the final condenser may be conducted oil to any suitable source through an outlet pipe26.

What ll claim and desire to secure by Let ters Patent of the United States is 11. The process which consists in treating an oxidized ore'of beryllium with carbon ran ' beryl with carbon and heat to produce a compound of beryllium and a member of the carbon group, and reacting upon said compound with gaseous hydrochloric acid to produce beryllium chlorid.

3. The process which consists in treating an oxidized ore of beryllium with carbon and heat to produce a compound of beryllium and a member of the carbon group, reacting upon said compound with gaseous hydrochloric acid to produce beryllium chlorid, and condensing the beryllium chlorid from the gaseous product.

4. The process which consists in treating an oxidized ore of beryllium with carbon and heat to produce a reduction product con taining beryllium, reacting upon said product with gaseous hydrochloric acid to produce volatile beryllium chlorid, and condensing said beryllium chlorid.

5. The process which consists in treating an oxidized ore of beryllium with carbon and heat to produce a reduction product containing beryllium, reacting upon said product with gaseous hydrochloric acid at a temperature below the sublimation temperature of ferrous chlorid and above the sublimation temperature of beryllium chlorid, and conducting away and condensing the volatilized beryllium chlorid.

6. The process which consists in treating an oxidized ore of beryllium with carbon and heat to produce a reduction product containing beryllium, reacting upon said product with gaseous hydrochloric acid at a temperature below the sublimation temperature of ferrous chlorid and above the sublimation temperature of beryllium chlorid, and conducting away and condensing the volatilized beryllium chlorid ,at a

temperature below the sublimation temperature of beryllium chlorid and above the sublimation temperature of aluminum chlorid.

7. The process which consists in treating an oxidized ore'of beryllium with carbon and heat to. produce a reduction product containing beryllium, reacting upon said product with gaseous hydrochloric acid at a temperature sufiicient to generate volatilized beryllium chlorid, and recovering such volatilized beryllium chlorid by fractional condensation.

8. The processwhich consists in treating an. oxidized ore of beryllium with carbon and heat to produce a reduction product containing beryllium, reacting upon said product with gaseous hydrochloric acid to produce volatilized beryllium chlorid, condensing the volatilized beryllium chlorid, and treating said chlorid with water to produce substantially pure beryllium oxid.,

9. The process which consists in treating an oxidized ore of beryllium with carbon and heat to produce a compound of beryl lium and a member of the carbon group, and

reacting uponsaid compound in pulverized form with gaseous hydrochloric acid to produce beryllium chlorid.

10. The process which consists in treating an oxidized ore of beryllium with carbon and heat to produce a compound of beryllium and a member of the carbon group, and reacting upon said compound with gaseous hydrochloric acid to produce beryllium chlorid by suspending said compound in pulverized form in said acid.

In testimony whereof I have hereunto signed my name in the presence of two subscribing witnesses.

' LOUIS BURGESS. Witnesses:

AGNES E. CUNNEEN, (J. Gr. HEYLMUN- 

